EP0490677A2 - Process for the production of cellulose ester fibrets - Google Patents
Process for the production of cellulose ester fibrets Download PDFInfo
- Publication number
- EP0490677A2 EP0490677A2 EP91311565A EP91311565A EP0490677A2 EP 0490677 A2 EP0490677 A2 EP 0490677A2 EP 91311565 A EP91311565 A EP 91311565A EP 91311565 A EP91311565 A EP 91311565A EP 0490677 A2 EP0490677 A2 EP 0490677A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- solvent
- cellulose ester
- weight percent
- fibrets
- acetone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
- 229920002678 cellulose Polymers 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 65
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 16
- 238000010008 shearing Methods 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229920002301 cellulose acetate Polymers 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 10
- 239000001913 cellulose Substances 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims 2
- 238000000926 separation method Methods 0.000 claims 2
- 239000011877 solvent mixture Substances 0.000 description 11
- 239000007921 spray Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005549 size reduction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 206010061592 cardiac fibrillation Diseases 0.000 description 1
- 229920006217 cellulose acetate butyrate Polymers 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000002600 fibrillogenic effect Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/40—Formation of filaments, threads, or the like by applying a shearing force to a dispersion or solution of filament formable polymers, e.g. by stirring
Definitions
- This invention relates to an improved process for the production of cellulose ester fibrets.
- this invention relates to a process for the production of cellulose ester fibrets wherein a solvent-nonsolvent mixture is recycled to the fibret precipitation zone.
- Short fibrillar cellulose ester material are employed in a variety of applications such as in the manufacture of tobacco smoke filters and as a replacement for clay and titanium dioxide in paper opacification.
- Fibrets can be produced using an unstable wet spinning process in which the fibrets are precipitated out of an organic solution of the polymer and formed, in a non-solvent, under controlled shearing conditions.
- the formed fibrets are in a mixture of the organic solvent and non-solvent.
- the mixture is then screened or filtered to increase the fibret concentration and the fibret concentrate thereafter heated to evaporate the organic solvent.
- the solvent is separated by distillation from the solvent-nonsolvent mixtures withdrawn from the screening or filtering and the fibret concentrate forming steps.
- Figure 1 is a schematic flow sheet of the process of the invention.
- a supply 10 of cellulose ester in a liquid mixture is prepared, such liquid mixture comprising two miscible components: an organic solvent such as acetone, methyl ethyl ketone, acetaldehyde or ethyl acetate and a miscible liquid non-solvent for the cellulose ester such as water, methanol or ethanol.
- the liquid non-solvent comprises from about 2 to about 20 percent by weight of the solvent and non-solvent mixture.
- the preferred organic solvent is acetone which is miscible with the preferred nonsolvent, water.
- the cellulose esters of this invention include cellulose acetate, cellulose triacetate, cellulose acetate butyrate, benzyl cellulose, or mixtures thereof with cellulose acetate being the preferred cellulose ester.
- the cellulose esters of this invention are prepared from an acetylation grade wood pulp with higher than 90 percent by weight of hemicellulose. It is also preferred that high purity cellulose esters be employed.
- the concentration of cellulose ester in the solvent and nonsolvent mixture should preferably be from about 5 to about 15 percent by weight with the particular concentration of the cellulose ester being dependent upon the method selected to form the fibrets.
- the cellulose ester, solvent and non-solvent mixture is then introduced into the precipitation non-solvent in a fibret precipitation zone under shearing conditions.
- the shearing high velocity of the non-solvent stream in the venturi throat region attenuates the cellulose ester-solvent mixture and additionally extracts the solvent, forming fibrets.
- concentration of the cellulose ester in the solvent and non-solvent mixture By changing the concentration of the cellulose ester in the solvent and non-solvent mixture, the flow rate of the solvent and nonsolvent mixture, or the temperature of the solvent and non-solvent mixture, the size, degree of fibrillation and length of the fibrets can be controlled.
- the term "fibret" as employed herein refers to a high surface area, cellulose ester fibrillar material having surface areas in excess of 5.0 square meters per gram, lengths of less than 1000 microns and diameters of from about 0.5 to 50 microns.
- Mineral additives such as titanium oxide, barium sulfate and aluminum oxide can be included in the cellulose ester-solvent mixture passed to the capillary needle. If included, the concentration of such additives can be up to 75 percent of the weight of the cellulose ester as part of the total solids.
- filter means 16 can comprise a commercially available screen which forms a thickened slurry of the fibrets passed via conduit 18 to a pressure vessel 19. A mixture of the solvent and non-solvent is withdrawn from filter means 16 via conduit 17.
- Saturated steam is introduced into pressure vessel 19 via conduit 20 at a rate so as to maintain the hereafter described temperature.
- the pressure within pressure vessel 19 is normally within the range of about 0 to about 15 pounds per square inch gauge (psig) and the temperature within the vessel is such as to separate substantially all of the remaining solvent from the fibrets at the vessel pressure.
- psig pounds per square inch gauge
- the pressure within vessel 19 is in the range of about 10 psig to about 12 psig and the temperature is in the range of about 220° to about 240°F.
- Vaporized solvent and non-solvent are withdrawn from pressure vessel 19 via conduit 21.
- the fully formed fibrets are withdrawn from pressure vessel 19 as a slurry in the non-solvent, normally less than 2.0 weight percent solids, via conduit 22 and passed to a homogenizer vessel 23 wherein size reduction of the large fibrets can be effected. Size reduction can be accomplished by passing the dilute slurry through a narrow orifice with a high pressure drop. After homogenization, the slurry can be passed via conduit 24 to a non-solvent separator 26, such as a centrifuge, wherein the non-solvent is separated from the fibrets.
- Product pill-free fibrets normally containing from about 65 to about 88 weight percent non-solvent are withdrawn from separator 26 via conduit 27.
- the product fibrets of the invention can be used as filter aids and in the production of heavy weight paper.
- the fibrets because of their pill-free characteristics are particularly suitable in the production of fine paper, filtration paper, and lightweight non-wovens applications.
- the solvent and non-solvent mixture withdrawn from filter means 16 via conduit 17 can be recycled to spray nozzle assembly 12 via conduit 13.
- the recycle stream can include the non-solvent stream withdrawn from separator 26 via conduit 25.
- Make-up non-solvent can be added to the recycle stream via conduit 29. If the non-solvent makeup is not water, the non-solvent withdrawn from pressure vessel 19 via conduit 22 and recycled via conduits 25 and 13 will comprise a mixture of water and makeup non-solvent.
- the recycle operation can be continued until the concentration of the solvent in conduit 13 is at least 7.5 weight percent, preferably at least 12.5 weight percent when the cellulose ester is cellulose acetate, the solvent is acetone and the non-solvent is water.
- concentration of solvent in conduit 17 becomes a maximum of 15.0 weight percent when the cellulose ester is cellulose acetate, the solvent is acetone and the non-solvent is water, a portion of the mixture withdrawn from filter means 17 via conduit 17 can be passed via conduit 28 to a conventional solvent recovery system.
- the invention is further illustrated by the following example.
- a cellulose acetate dope comprising 10.0 weight percent cellulose acetate, 81.1 weight percent acetone and 9.0 weight percent water was passed to spray nozzle assembly 12 via conduit 11.
- a recycle stream comprising 7.5 weight percent acetone and 92.5 weight percent water was passed via conduit 13 to spray nozzle assembly 12.
- a dilute fibret slurry comprising 0.44 weight percent cellulose acetate fibrets, 3.54 weight percent acetone and 96.2 weight percent water was passed to filter means 16.
- the slurry concentrate withdrawn from filter means 16 and passed to pressure vessel 19 via conduit 18 comprised 2.00 weight percent cellulose acetate fibrets, 3.54 weight percent acetone and 94.46 weight percent water.
- the liquid stream withdraw from filter means 16 and recycled via conduits 17 and 13 to spray nozzle assembly 12 comprised 10.0 weight percent acetone and 90.0 weight percent water.
- Saturated steam was introduced into pressure vessel 19 via conduit 20 at a rate and temperature so as to achieve and maintain a temperature in vessel 19 of 230°F.
- Vessel 19 was pressurized to a pressure of 10 psig.
- a vaporized stream comprising 12.2 weight percent acetone and 87.8 weight percent water was withdrawn from vessel 19 via conduit 21.
- the fibret slurry withdrawn from vessel 19 via conduit 22 comprised 1.94 weight percent cellulose acetate and 98.06 weight percent water and was substantially free of chips and pills.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
Description
- This invention relates to an improved process for the production of cellulose ester fibrets. In another aspect this invention relates to a process for the production of cellulose ester fibrets wherein a solvent-nonsolvent mixture is recycled to the fibret precipitation zone.
- Short fibrillar cellulose ester material (termed fibrets) are employed in a variety of applications such as in the manufacture of tobacco smoke filters and as a replacement for clay and titanium dioxide in paper opacification. Fibrets can be produced using an unstable wet spinning process in which the fibrets are precipitated out of an organic solution of the polymer and formed, in a non-solvent, under controlled shearing conditions. The formed fibrets are in a mixture of the organic solvent and non-solvent. The mixture is then screened or filtered to increase the fibret concentration and the fibret concentrate thereafter heated to evaporate the organic solvent. The solvent is separated by distillation from the solvent-nonsolvent mixtures withdrawn from the screening or filtering and the fibret concentrate forming steps.
- In the precipitation step, a large volume of non-solvent is required which must be heated. Additionally, large distillation capacity is required to separate the solvent from the non-solvent in the mixtures of such solvent and non-solvent withdrawn from the filter and fibret concentration steps. Thus, it would be desirable to reduce the energy and capital costs associated with the precipitation and subsequent distillation steps.
- In the production of cellulose ester fibrets by precipitation of the fibrets from a solvent solution of such fibrets into a non-solvent, an improved process is provided whereby the solvent-nonsolvent mixtures separated from the product fibrets is recycled to the precipitation zone. Preferably, such recycle is continued until the concentration of solvent in the recycle stream is at least 10.0 weight percent.
- Figure 1 is a schematic flow sheet of the process of the invention.
- Referring to Figure 1, a
supply 10 of cellulose ester in a liquid mixture is prepared, such liquid mixture comprising two miscible components: an organic solvent such as acetone, methyl ethyl ketone, acetaldehyde or ethyl acetate and a miscible liquid non-solvent for the cellulose ester such as water, methanol or ethanol. The liquid non-solvent comprises from about 2 to about 20 percent by weight of the solvent and non-solvent mixture. The preferred organic solvent is acetone which is miscible with the preferred nonsolvent, water. - The cellulose esters of this invention include cellulose acetate, cellulose triacetate, cellulose acetate butyrate, benzyl cellulose, or mixtures thereof with cellulose acetate being the preferred cellulose ester. Preferably, the cellulose esters of this invention are prepared from an acetylation grade wood pulp with higher than 90 percent by weight of hemicellulose. It is also preferred that high purity cellulose esters be employed.
- The concentration of cellulose ester in the solvent and nonsolvent mixture should preferably be from about 5 to about 15 percent by weight with the particular concentration of the cellulose ester being dependent upon the method selected to form the fibrets. The cellulose ester, solvent and non-solvent mixture is then introduced into the precipitation non-solvent in a fibret precipitation zone under shearing conditions.
- A suitable method for producing the fibrets is described in U.S. 4,192,838 which is incorporated herein by reference thereto. When employing the spray nozzle described therein, the cellulose ester dissolved in the solvent mixture is passed at an elevated temperature and under pressure via
line 11 through a capillary needle ofspray nozzle assembly 12 situated in the throat of a venturi tube through which a coagulation heated nonsolvent and solvent mixture as subsequently described is passed fromconduit 13. The temperatures of the feeds to the spray nozzle assembly will be dependent upon the selected ester, solvent and non-solvent. When employing cellulose acetate, acetone and water, the temperature in the spray nozzle assembly will normally range from 120°F to 170°F. - The shearing high velocity of the non-solvent stream in the venturi throat region attenuates the cellulose ester-solvent mixture and additionally extracts the solvent, forming fibrets. By changing the concentration of the cellulose ester in the solvent and non-solvent mixture, the flow rate of the solvent and nonsolvent mixture, or the temperature of the solvent and non-solvent mixture, the size, degree of fibrillation and length of the fibrets can be controlled. The term "fibret" as employed herein refers to a high surface area, cellulose ester fibrillar material having surface areas in excess of 5.0 square meters per gram, lengths of less than 1000 microns and diameters of from about 0.5 to 50 microns.
- Another suitable method of producing the fibrets is described in U.S. 4,047,862, also incorporated herein by reference thereto. As described therein the cellulose acetate, solvent and non-solvent mixture is extruded through an orifice into a heated region of shear and high draw in a precipitation bath containing a non-solvent for the ester.
- Mineral additives such as titanium oxide, barium sulfate and aluminum oxide can be included in the cellulose ester-solvent mixture passed to the capillary needle. If included, the concentration of such additives can be up to 75 percent of the weight of the cellulose ester as part of the total solids.
- The fibrets as a dilute slurry in the solvent and non-solvent mixture is passed via
conduit 14 to a filter means 16. Suitably, filter means 16 can comprise a commercially available screen which forms a thickened slurry of the fibrets passed viaconduit 18 to apressure vessel 19. A mixture of the solvent and non-solvent is withdrawn from filter means 16 viaconduit 17. - Saturated steam is introduced into
pressure vessel 19 viaconduit 20 at a rate so as to maintain the hereafter described temperature. The pressure withinpressure vessel 19 is normally within the range of about 0 to about 15 pounds per square inch gauge (psig) and the temperature within the vessel is such as to separate substantially all of the remaining solvent from the fibrets at the vessel pressure. Normally, when producing cellulose acetate fibrets from an acetone-water mixture the pressure withinvessel 19 is in the range of about 10 psig to about 12 psig and the temperature is in the range of about 220° to about 240°F. Vaporized solvent and non-solvent are withdrawn frompressure vessel 19 viaconduit 21. - The fully formed fibrets, substantially free of solvent, are withdrawn from
pressure vessel 19 as a slurry in the non-solvent, normally less than 2.0 weight percent solids, viaconduit 22 and passed to ahomogenizer vessel 23 wherein size reduction of the large fibrets can be effected. Size reduction can be accomplished by passing the dilute slurry through a narrow orifice with a high pressure drop. After homogenization, the slurry can be passed via conduit 24 to anon-solvent separator 26, such as a centrifuge, wherein the non-solvent is separated from the fibrets.
Product pill-free fibrets, normally containing from about 65 to about 88 weight percent non-solvent are withdrawn fromseparator 26 viaconduit 27. - The product fibrets of the invention can be used as filter aids and in the production of heavy weight paper. The fibrets because of their pill-free characteristics are particularly suitable in the production of fine paper, filtration paper, and lightweight non-wovens applications.
- The solvent and non-solvent mixture withdrawn from filter means 16 via
conduit 17 can be recycled to spraynozzle assembly 12 viaconduit 13. Optionally, the recycle stream can include the non-solvent stream withdrawn fromseparator 26 via conduit 25. Make-up non-solvent can be added to the recycle stream viaconduit 29. If the non-solvent makeup is not water, the non-solvent withdrawn frompressure vessel 19 viaconduit 22 and recycled viaconduits - The recycle operation can be continued until the concentration of the solvent in
conduit 13 is at least 7.5 weight percent, preferably at least 12.5 weight percent when the cellulose ester is cellulose acetate, the solvent is acetone and the non-solvent is water. When the concentration of solvent inconduit 17 becomes a maximum of 15.0 weight percent when the cellulose ester is cellulose acetate, the solvent is acetone and the non-solvent is water, a portion of the mixture withdrawn fromfilter means 17 viaconduit 17 can be passed viaconduit 28 to a conventional solvent recovery system. - The invention is further illustrated by the following example.
- A cellulose acetate dope comprising 10.0 weight percent cellulose acetate, 81.1 weight percent acetone and 9.0 weight percent water was passed to
spray nozzle assembly 12 viaconduit 11. A recycle stream comprising 7.5 weight percent acetone and 92.5 weight percent water was passed viaconduit 13 to spraynozzle assembly 12. - A dilute fibret slurry comprising 0.44 weight percent cellulose acetate fibrets, 3.54 weight percent acetone and 96.2 weight percent water was passed to filter means 16. The slurry concentrate withdrawn from filter means 16 and passed to
pressure vessel 19 viaconduit 18 comprised 2.00 weight percent cellulose acetate fibrets, 3.54 weight percent acetone and 94.46 weight percent water. The liquid stream withdraw from filter means 16 and recycled viaconduits nozzle assembly 12 comprised 10.0 weight percent acetone and 90.0 weight percent water. - Saturated steam was introduced into
pressure vessel 19 viaconduit 20 at a rate and temperature so as to achieve and maintain a temperature invessel 19 of 230°F. Vessel 19 was pressurized to a pressure of 10 psig. A vaporized stream comprising 12.2 weight percent acetone and 87.8 weight percent water was withdrawn fromvessel 19 viaconduit 21. The fibret slurry withdrawn fromvessel 19 viaconduit 22 comprised 1.94 weight percent cellulose acetate and 98.06 weight percent water and was substantially free of chips and pills. - Although the invention has been described in detail with respect to specific embodiments, it should be noted that this invention is by no means limited to those specific embodiments.
- The dependencies of the subsidiary claims hereinafter do not imply any limitation as to the possible combinations of the features mentioned in those claims.
Claims (13)
- In a process which comprises contacting a solution of a cellulose ester with a non-solvent for the cellulose ester in a cellulose ester precipitation zone under shearing conditions, and thereafter separating a solvent-nonsolvent mixture from the formed fibrets; the improvement which comprises recycling the separated solvent-nonsolvent mixture to said precipitation zone.
- The process of claim 1 wherein said solution contains from about 5 to about 15 weight percent cellulose ester.
- The process of claim 2 wherein said solution contains from about 2 to about 20 weight percent non-solvent.
- The process of claim 3 wherein said cellulose ester is cellulose acetate, solvent is acetone, and said non-solvent is water.
- The process of claim 4 wherein the recycled solvent-nonsolvent mixture contains at least 10.0 weight percent acetone.
- In a process which comprises contacting a solution of a cellulose ester with a non-solvent for the cellulose ester in a cellulose ester precipitation zone under shearing conditions, separating a solvent-nonsolvent mixture from a thickened slurry of the formed fibrets, and separating the solvent from the thickened fibret slurry in a pressurized separation zone; the improvement which comprises recycling said solvent-nonsolvent mixture and said solvent withdrawn from said pressure separation zone to said cellulose ester precipitation zone.
- The process of claim 6 wherein said solution contains from about 5 to about 15 weight percent cellulose ester.
- The process of claim 7 wherein said solution contains from about 2 to about 20 weight percent non-solvent.
- The process of claim 8 wherein said cellulose ester is cellulose acetate, said solvent is acetone, and said non-solvent is water.
- The process of claim 9 wherein the concentration of acetone in the total recycle stream to said precipitation zone is at least 10.0 weight percent.
- The process of claim 10 wherein the concentration of acetone in said solvent-nonsolvent mixture does not exceed 15.0 weight percent.
- A process which comprises contacting a solution of a cellulose ester with a non-solvent for the cellulose ester in a cellulose precipitation zone under shearing conditions, said nonsolvent containing at least 7.5 weight percent of the solvent contained in said solution of said cellulose ester.
- The process of claim 12 wherein said cellulose ester is cellulose acetate, said solvent is acetone and said non-solvent is water.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US07/627,279 US5071599A (en) | 1990-12-14 | 1990-12-14 | Process for the production of cellulose ester fibrets |
US627279 | 1990-12-14 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0490677A2 true EP0490677A2 (en) | 1992-06-17 |
EP0490677A3 EP0490677A3 (en) | 1992-12-09 |
Family
ID=24514004
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP19910311565 Ceased EP0490677A3 (en) | 1990-12-14 | 1991-12-12 | Process for the production of cellulose ester fibrets |
Country Status (3)
Country | Link |
---|---|
US (1) | US5071599A (en) |
EP (1) | EP0490677A3 (en) |
JP (1) | JPH04263610A (en) |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3420359B2 (en) * | 1994-10-21 | 2003-06-23 | ダイセル化学工業株式会社 | Filter material for tobacco smoke, fibrous cellulose ester and method for producing the same |
US5695647A (en) * | 1996-04-19 | 1997-12-09 | North Carolina State University | Methods of treating wastewater |
DE19616010C2 (en) * | 1996-04-23 | 1998-07-09 | Seitz Filter Werke | Process and device for the production of fibrets (fibrids) from cellulose derivatives |
GB9800850D0 (en) | 1998-01-15 | 1998-03-11 | Courtaulds Plc | Methods of manufacturing and collecting cellulosic particles |
US6168733B1 (en) | 1998-08-31 | 2001-01-02 | Eastman Chemical Company | Method for forming discrete pellets from viscous materials |
US6184373B1 (en) | 1999-09-03 | 2001-02-06 | Eastman Chemical Company | Method for preparing cellulose acetate fibers |
JP5165427B2 (en) * | 2007-03-23 | 2013-03-21 | 富士フイルム株式会社 | Solution casting method |
JP5982412B2 (en) * | 2014-02-12 | 2016-08-31 | 富士フイルム株式会社 | Fiber manufacturing method, nonwoven fabric manufacturing method, fiber manufacturing facility and nonwoven fabric manufacturing facility |
CN110250568A (en) * | 2019-06-13 | 2019-09-20 | 上海洁晟环保科技有限公司 | A kind of purposes of cellulose diacetate pulp as cigarette filter stick |
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US4040856A (en) * | 1975-06-17 | 1977-08-09 | Crown Zellerbach Corporation | Production of discrete cellulose acetate fibers by emulsion flashing |
US4047862A (en) * | 1975-10-24 | 1977-09-13 | Celanese Corporation | Cellulose ester fibrillar structure |
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US3042970A (en) * | 1961-08-14 | 1962-07-10 | American Cyanamid Co | Particulation of polymer by extruding a solution thereof into a liquid stream of fluid |
JPS497518A (en) * | 1972-05-31 | 1974-01-23 | ||
US3961007A (en) * | 1973-10-23 | 1976-06-01 | E & J Gallo Winery | Continuous process for making fibrous cellulose acetate filter material |
US4205025A (en) * | 1975-12-22 | 1980-05-27 | Champion International Corporation | Synthetic polymeric fibrids, fibrid products and process for their production |
US4192838A (en) * | 1976-10-06 | 1980-03-11 | Celanese Corporation | Process for producing filter material |
JPS6240456A (en) * | 1985-08-16 | 1987-02-21 | Konishiroku Photo Ind Co Ltd | Silver halide photographic sensitive material |
-
1990
- 1990-12-14 US US07/627,279 patent/US5071599A/en not_active Expired - Lifetime
-
1991
- 1991-12-12 EP EP19910311565 patent/EP0490677A3/en not_active Ceased
- 1991-12-13 JP JP3330348A patent/JPH04263610A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3441473A (en) * | 1966-03-16 | 1969-04-29 | West Virginia Pulp & Paper Co | Cellulose derivative compositions and paper containing the derivatives |
US4040856A (en) * | 1975-06-17 | 1977-08-09 | Crown Zellerbach Corporation | Production of discrete cellulose acetate fibers by emulsion flashing |
US4047862A (en) * | 1975-10-24 | 1977-09-13 | Celanese Corporation | Cellulose ester fibrillar structure |
Also Published As
Publication number | Publication date |
---|---|
JPH04263610A (en) | 1992-09-18 |
US5071599A (en) | 1991-12-10 |
EP0490677A3 (en) | 1992-12-09 |
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